CN101298506B - PVC plasticiser synthesized by using benzoic anhydride by-product and maize mixed alcohol - Google Patents
PVC plasticiser synthesized by using benzoic anhydride by-product and maize mixed alcohol Download PDFInfo
- Publication number
- CN101298506B CN101298506B CN2008100286395A CN200810028639A CN101298506B CN 101298506 B CN101298506 B CN 101298506B CN 2008100286395 A CN2008100286395 A CN 2008100286395A CN 200810028639 A CN200810028639 A CN 200810028639A CN 101298506 B CN101298506 B CN 101298506B
- Authority
- CN
- China
- Prior art keywords
- product
- benzoic anhydride
- mixed alcohol
- anhydride
- phthalic anhydride
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a PVC plasticizer synthesized from phthalic anhydride by-product and corn mixed alcohol, which is characterized in that the product is prepared under the effect of organic tin catalysts, basing on raw materials of phthalic anhydride by-product and corn alcohol produced during phthalic anhydride production; the invention not only can resolve the problem of recycling of distillation light fraction generated during phthalic anhydride production to prevent environmental pollution and can decrease investment for recycling of distillation light fraction to reduce cost of theplasticizer, but also can fully use biological energy source to remedy influence of crude oil price to the product and give a motivation for exploitation of application field of biological energy source.
Description
Technical field
The present invention relates to a kind of softening agent, particularly a kind of softening agent that is used for plastifying synthetic resins such as PVC.
Background technology
Softening agent all is widely used in many fields such as PVC plastic working, synthetic rubber, coating, tackiness agent, chemical industry are synthetic.The kind of conventional plasticizers is a lot, the higher and not environmental protection of these softening agent ubiquity costs shortcoming.In addition; in the phthalic anhydride production process, can produce a certain amount of distillation light fraction---by-product of benzoic anhydride; include a certain amount of phthalic anhydride and phenylformic acid in these distillation light fractions; as directly with its discharging; phthalic anhydride and phenylformic acid in the distillation light fraction can cause severe contamination to environment, and also can cause the waste of resource, therefore are the protection environment; the saving data need be recycled the distillation light fraction.Traditional method that the distillation light fraction is recycled is that the distillation light fraction is collected, and uses as the phthalic anhydride raw materials for production after treatment.The technology of this recycling is complicated, and facility investment is more, and cost recovery is higher.In addition, change along with international oil price, the cost of organic chemical industry's product presents unsteady significantly, and, under current form, the exploitation of bioenergy and utilization have become international trend. and China's bioenergy exploitation has obtained outstanding achievement, but its Application Areas also needs more to be developed. for addressing the above problem, be necessary to develop a kind of new softening agent, be intended to utilize the distillation light fraction and the bioenergy maize mixed alcohol that in the phthalic anhydride production process, produce to be raw material, like this, can reduce the investment that the distillation light fraction is recycled, reduce the cost of product, and can guarantee the stable of quality product, can prevent the pollution of the environment again, meet the trend of international energy development.
Summary of the invention
In order to overcome the deficiencies in the prior art, the invention provides a kind of with by-product of benzoic anhydride and maize mixed alcohol synthetic PVC softening agent, this softening agent has the low characteristics of cost, and one of its raw material derives from the by product in the phthalic anhydride production, thereby can prevent the pollution of the environment, and can reduce the investment that the distillation light fraction is recycled, another raw material is a bioenergy, has good social benefit.
The technical solution adopted for the present invention to solve the technical problems is:
With by-product of benzoic anhydride and maize mixed alcohol synthetic PVC softening agent, it is characterized in that it is is raw material with the by-product of benzoic anhydride and the maize mixed alcohol that produce in the phthalic anhydride production process, the product that under the organic tin catalyst action, is prepared from.
Include dibasic alcohol such as propylene glycol, ethylene glycol and butyleneglycol in the above-mentioned maize mixed alcohol, include diprotic acid such as phthalic anhydride and phenylformic acid in the by-product of benzoic anhydride; And by-product of benzoic anhydride, maize mixed alcohol mass fraction are respectively: 2.5～3.3 parts of by-product of benzoic anhydride, 1 part of maize mixed alcohol, organic tin catalyst levels are 85～120ppm of raw material gross weight.
Consist predominantly of phthalic anhydride and phenylformic acid in the by-product of benzoic anhydride that the present invention adopts, wherein phthalic anhydride accounts for 5%～50% of by-product of benzoic anhydride gross weight.
Organic tin catalyzer of the present invention can adopt tin oxalate, stannous octoate or the like.
Softening agent outward appearance of the present invention is dark-brown liquid, acid value (KOH-mg/g)≤1, hydroxyl valency (KOH-mg/g)≤9, viscosity (cps, 25 ℃) 100～200, proportion (20/20 ℃) 1.1～1.2, thermogravimetric loss (%)≤0.5.
The present invention can be prepared as follows: get by-product of benzoic anhydride and maize mixed alcohol and mix, add the organic tin catalyzer, reaction is warming up to 85 ℃～100 ℃ early stage, by-product of benzoic anhydride is dissolved fully, to prevent the phenylformic acid distillation in the by-product of benzoic anhydride, and kept 2～4 hours, and then normally heat up 210～230 ℃, to heat up in a steamer a temperature be 90～95 ℃ in control in the reaction process, react to acid value when qualified, begin to vacuumize, up to the qualified PVC softening agent that can obtain of every index of product with the by-product of benzoic anhydride modification.
The invention has the beneficial effects as follows: the present invention adopt the distillation light fraction that produces in the phthalic anhydride production process and environmental protection cheaply maize mixed alcohol be raw material, both can solve the recycling problem of the distillation light fraction that produces in the phthalic anhydride production process, prevent the pollution of the environment, reduce the investment that the distillation light fraction is recycled, expand the Application Areas of bioenergy, can reduce the cost of softening agent again.
The present invention is further described below in conjunction with embodiment.
Embodiment
Embodiment 1
Getting phthalic anhydride content and be 8% by-product of benzoic anhydride 1300 grams, maize mixed alcohol 520 grams mixes, add organic tin catalyzer 0.27 gram, reaction is warming up to 85 ℃～100 ℃ with it earlier early stage, by-product of benzoic anhydride is dissolved fully, and prevent that the phenylformic acid in the by-product of benzoic anhydride from distilling, and kept 2～4 hours, and then normally heat up 210～230 ℃, to heat up in a steamer a temperature be 90～95 ℃ in control in the reaction process, react to acid value when qualified, begin to vacuumize, up to the qualified PVC softening agent that promptly obtains with the by-product of benzoic anhydride modification of every index of product.
Embodiment 2
Get phthalic anhydride content and be 15.8 kilograms of mixing of 40 kilograms of by-product of benzoic anhydride, maize mixed alcohol of 20%, add 0.008 kilogram of organic tin catalyzer, reaction is warming up to 85 ℃～100 ℃ with it earlier early stage, by-product of benzoic anhydride is dissolved fully, and prevent that the phenylformic acid in the by-product of benzoic anhydride from distilling, and kept 2～4 hours, and then normally heat up 210～230 ℃, to heat up in a steamer a temperature be 90～95 ℃ in control in the reaction process, react to acid value when qualified, begin to vacuumize, up to qualified can the obtaining of every index of product with by-product of benzoic anhydride modified PVC softening agent.
Embodiment 3
Get phthalic anhydride content and be 30 kilograms of mixing of 66 kilograms of by-product of benzoic anhydride, maize mixed alcohol of 40%, add 0.01 kilogram of organic tin catalyzer, reaction is warming up to 85 ℃～100 ℃ with it earlier early stage, by-product of benzoic anhydride is dissolved fully, and prevent that the phenylformic acid in the by-product of benzoic anhydride from distilling, and kept 2～4 hours, and then normally heat up 210～230 ℃, to heat up in a steamer a temperature be 90～95 ℃ in control in the reaction process, react to acid value when qualified, begin to vacuumize, up to qualified can the obtaining of every index of product with by-product of benzoic anhydride modified PVC softening agent.
Claims (4)
1. with by-product of benzoic anhydride and maize mixed alcohol synthetic PVC softening agent, it is characterized in that it is is raw material with the by-product of benzoic anhydride and the renewable raw material maize mixed alcohol of growing that produce in the phthalic anhydride production process, the product that under the organic tin catalyst action, is prepared from.
2. according to claim 1 with by-product of benzoic anhydride and maize mixed alcohol synthetic PVC softening agent, it is characterized in that including in the described maize mixed alcohol propylene glycol, ethylene glycol and butyleneglycol; Include phthalic anhydride and phenylformic acid in the by-product of benzoic anhydride, and the mass fraction of by-product of benzoic anhydride, maize mixed alcohol is respectively: 2.5～3.3 parts of by-product of benzoic anhydride, 1 part of maize mixed alcohol, the organic tin catalyst levels is 85～120ppm of raw material gross weight.
3. by-product of benzoic anhydride and the maize mixed alcohol synthetic PVC softening agent used according to claim 1 and 2 is characterized in that consisting predominantly of in the by-product of benzoic anhydride phthalic anhydride and phenylformic acid, and wherein phthalic anhydride accounts for 5%～50% of by-product of benzoic anhydride gross weight.
4. according to claim 1 and 2 with by-product of benzoic anhydride and maize mixed alcohol synthetic PVC softening agent, it is characterized in that this softening agent outward appearance is dark-brown liquid, acid value≤1KOH-mg/g, hydroxyl valency≤9KOH-mg/g, viscosity 100～200cps in the time of 25 ℃, proportion 1.1～1.2 under 20/20 ℃ of condition, thermogravimetric loss≤0.5%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100286395A CN101298506B (en) | 2008-06-05 | 2008-06-05 | PVC plasticiser synthesized by using benzoic anhydride by-product and maize mixed alcohol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100286395A CN101298506B (en) | 2008-06-05 | 2008-06-05 | PVC plasticiser synthesized by using benzoic anhydride by-product and maize mixed alcohol |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101298506A CN101298506A (en) | 2008-11-05 |
| CN101298506B true CN101298506B (en) | 2010-12-08 |
Family
ID=40078468
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008100286395A Expired - Fee Related CN101298506B (en) | 2008-06-05 | 2008-06-05 | PVC plasticiser synthesized by using benzoic anhydride by-product and maize mixed alcohol |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101298506B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101875609B (en) * | 2010-06-04 | 2013-04-10 | 镇江联成化学工业有限公司 | Method for preparing PVC plasticizer from by-products of production of fumaric acid and recovery alcohol |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1065859A (en) * | 1991-04-13 | 1992-11-04 | 中国石油化工总公司巴陵石油化工公司 | The method that raw phthalic anhydride is recycled |
| CN1640866A (en) * | 2004-01-16 | 2005-07-20 | 湖南科技大学 | Method for preparing phthalic acid C4-C5 mixed ester using crude benzoic acid anhydride and alcohol oil |
-
2008
- 2008-06-05 CN CN2008100286395A patent/CN101298506B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1065859A (en) * | 1991-04-13 | 1992-11-04 | 中国石油化工总公司巴陵石油化工公司 | The method that raw phthalic anhydride is recycled |
| CN1640866A (en) * | 2004-01-16 | 2005-07-20 | 湖南科技大学 | Method for preparing phthalic acid C4-C5 mixed ester using crude benzoic acid anhydride and alcohol oil |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101298506A (en) | 2008-11-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104496819B (en) | A kind of method that environment-friendly plasticizer is prepared in waste resource recycling | |
| CN102731755B (en) | Method for preparing plasticizer | |
| CN110078903A (en) | A method of continuously preparing Biodegradable resin side by side | |
| CN101591588A (en) | The method of organic rhenium oxide-urea peroxide catalytic preparation epoxy soybean oil or epoxyfatty acid first (second) ester | |
| CN103668539B (en) | A kind of Antistatic type biomass polyester fiber and preparation method thereof | |
| CN105838047A (en) | Biodegradable modified lignin particles and production method thereof | |
| CN102604053B (en) | Method for preparing biomass polyester | |
| CN105038262A (en) | Environment-friendly regenerable softener and preparation method thereof | |
| CN103013682A (en) | Synthetic method for epoxy soybean oil acrylate | |
| CN114736507B (en) | Preparation method of biomass-based modified aldehyde-free environment-friendly artificial board adhesive | |
| CN102964495A (en) | Synthetic method of terpene resin | |
| CN104031153B (en) | A kind of catalyzed with solid supported heteropolyacid prepares the method for Starch rice acetic ester | |
| CN113735705B (en) | Method for catalyzing waste PET (polyethylene terephthalate) polyester to carry out methanol alcoholysis by polyion liquid | |
| CN101298506B (en) | PVC plasticiser synthesized by using benzoic anhydride by-product and maize mixed alcohol | |
| CN101307138B (en) | Unsaturated polyester resin modified by by-product of benzoic anhydride | |
| CN108219193A (en) | A kind of application of the preparation method of mixed plasticizer and its mixed plasticizer obtained | |
| CN101525477B (en) | Nanometer composite material of polyester and inorganic silicate | |
| CN104592024A (en) | Alcoholysis recovery method for waste polylactic acid material | |
| CN101948449A (en) | Method for preparing chloro-epoxy fatty acid methyl ester plasticizer | |
| CN102491900A (en) | Method for preparing diethylene glycol dibenzoate | |
| CN103668538B (en) | A kind of ultraviolet-resisting biomass polyester fiber and preparation method thereof | |
| CN108675920A (en) | A kind of method that solvent-free quick oxicracking epoxy aliphatic acid methyl ester prepares aldehyde material | |
| CN110804029B (en) | Epoxy plasticizer and preparation method thereof | |
| CN1778858A (en) | Biomass-base and waterproof wooden adhesive without formaldehyde and its production | |
| CN106188144B (en) | A kind of liquid organotin antimonial and its preparation method and application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20101208 Termination date: 20180605 |